Method for drying solids



July 17, 1934. R. D. MYERS METHOD FOR DRYING SOLIDS Original Filed June 25, 1929 INVENTOR. R0//a/7d Q Myers WM 52 We, A

A TTORNEY.

Patented July l7, 1934 p uror-13D STATES: PATENT OFFICE v v i ;;1',96,4 6;. I

METHOD FOR, DRYING-soups A Rolland'DlMyers, Edgewood Arsenal, Md. original application June 25, 1929, Serial No.

' 373,674. Divided and this application August 2,1932, Serial No; 627,246.J ,m

H A 3150mm. (c a -i16 7, fiGr-finted underthe act of-March '3,- 1883;

The-invention describedherein maybe manufactured and used by or for the Government-for governmental purposes,without the payment to me of any royaltythereon.

-Thisinve'ntion relates in general toremoving contained liquids fromvolatile solids having a low intersolubilitytherewith in the liquid phase, and more particularly has referenceto a'process and apparatus for drying hexachlorethanei Previous to this Itim'e, the various methods employed for removing contained liquids from materials of'this character have not usually proved well suited for practical purposes In the 'pastfit has been customary in drying solids, of the type of-hexachlorethane for example, to

centrifuge the; wet material to reduce the mois ture content to aslow a degree as practical.

The remaining'trace's ofwater-have been removed to the greatest possible extent by bringing the material in contact with relatively dry air. In carrying on an air-drying operation of this type, however; a large percentage of 1 the solid under treatment is lost-ranging in many instances from an'approximate of around-ten to over fifteen percent. 7 An object of this invention is to provide a process and apparatus for removing contained liquids from volatile solids having a low'intersolubility therewith in the liquid phase without any appreciable loss of the normally solidmaterial; 7 a V 1 Another object of this inventionis to provide a process and apparatus for removing contained liquids from volatile solids having a'low intersolubility therewith in the liquid phase-without anyappreciable loss of the normally solid material in which the contained liquid'is separated and'removecl- 1 Still another object of this invention is to provide-a process and apparatus for removing contained liquids from volatile solidshaving' a low intersolubility"therewith in; theliquid phase without any appreciable loss'of' the normally solid material in which the solid is separated in the liquid phase and removeds 4 A' further object of this inventionis to provide a process of drying hexachlorethane without any appreciable loss of' the material.

This invention contemplates in general remov-' ingcontained liquidsirom volatile solids'having a' low intersolubility. therewith-in the 'liquid' phase: by 'liquefying the solid: in a closed vessel and efiecting'agseparation of theliquid layers sotasztorobtain a productsubstantially free from jamendedlApl il 30, 19 28 370 0. G. 757) 7' With these and other objects in view which mayjbeincident to myimprovements, the invention consists in the parts and'combinations to behereinafter set forth vand. claimed, with the understanding that the severalxnecessary elements comprising my invention may be varied in, construction, proportions and arrangement, without departingfrom the spirit and scope of r the appended claims.

In order to make my invention more= clearly understood,.I have shown in the accompanying drawings. means for carrying the same into prac-' tical effect; without limiting the improvements in their-useful applications to the particular constructions which for: the purpose of explanation have been made the subject, of illustration.

This application is-a division of my application for Method andapparatus for; dryinghexachlorethane, Serial .Number 373,674,; filed June 25,1929., V v

Figure 1 is a sectional view of one form of apparatusin which the contained liquid may be decanted andthe'normally solid material drawn oil in the liquid phase.

Referring by numerals to the drawing, there is shown. one 'form of apparatus a suitable for carrying on the process of this invention which will be" described with reference to one specif c application ,of' the invention for the drying 'of hexachlo'rethane Thisapparatu's comprises" a plurality of superimposed containers 35 .an'd 36, having jackets 37 and 38iormed integral there-f withas shown; The lower jacket isprovided with an'outlet' 39 at the'bottorn'and .an inlet 41 at the top,"and jacket 38 is likewise provided with aibottom'outlet 42 and a topvinlet, 43.

, A member '44 formed of a bowl sh aped' plate 45 backed againsta bowl, shapedplate 46 and having a central aperture'47,isinterposed be tween the oontainersgso that itv acts as a bottomclos ure for the f'upperfcontainer 3 6jan'd a top. closure for the'lower' container 35"., The member 44 is provided in addition with an outer jacket 48 having va plurality of outlets 49 and 51 therein. V

- The lower"'container"35, is provided with p a bottom closure 52 having a conduit 53 formed on one side thereof, adapted to receive; an outlet line. The upper container "36 is: provided with a domesh'aped closure 54 having a central aper-.' ture th'rough' which is inserted a r0d"55 A pentrally located tubular extension 56 having an outwardly flangedtop 5'7 is formed on the zclosf' ure '54. A 'stuflingg'land '58 is adapt edjto be ,i

serted over therod 55 and seated in the tubalar extension 56, which is provided with packing 59. A tapered extension 61 formed integral with the stuffing gland having a centrally threaded aperture is mounted on the top of the stufiing gland adapted to be engaged by threads 62 formed on the end of rod 55.

It will be noted that the rod extends through the central aperture 47 in the member 44. A plug 63 composed of any suitable material not affected by the substances charged into the containers is mounted on the end of the rod and held by a nut 64. A wheel 65 is fixed on the upper end of the rod 55 so that by rotating the same communication between the two containers may be stopped by the plug 63 stopping the aperture 47. V

The dome cover 54 is provided in addition with an upwardly extending tubular extension 66 having a flanged top 67, through which ma-- terial for treatment is charged, and provided with a closure 68 preferably slidably secured thereon by a bolt 69. In the preferred construction, it will be noted that the closure 68 may be held in the opposite side by insertion in a groove provided in the side of the extension 56.

--; it is desired to remove contained. liquids.

It will be apparent, however, that the closure 68 may be fixed over the opening in any other suitable manner so that it may be conveniently removed and replaced.

The jacket 38- on the upper container is connected to the jacket 48 on the member 44 to an elbowed line '71 connected to the outlets. 42 and 49 and the jacket 48 connected to the 1 jacket 37 on the lower container through a similar line 72 connected to the outlets 51 and 41. A suitable heating medium, such. as oil, is preferably charged through the inlet 43 so that it will circulate about the upper container, the member 44 and the lower container, and out of the outlet 39 to heat the contents of the apparatus.

A pipe '73 having a tapered mouth 74 is positioned in the upper container, having an elbow extending through a packing gland 75 in the wall of the container. It is intended that the pipe be rotated in the gland to draw oil liquids from different levels within the container, a valve and rotating means (not shown) being provided on the outside. The bowl shaped plate 46 is provided with an aperture '76 in which is connected a pressure inlet line 77, which forces material in the lower container out of the conduit 53. A valve 78 is interposed in the line '77 to control the admission of the agent employed, which is preferably air.

This apparatus may be provided with the usual temperature and pressure indicating means, such as a thermometer and a pressure gauge, as well as a pressurecontrol valve of conventional type. It may also be desirable to provide a well with a sight glass therein as shown in Fig. 1 of application No. 373,674, of which this application is a division, to allow observation of the liquid levels therein when it is desired to draw off a certain quantity of liquid through pipe '73.

This apparatus is suitable for hexachlorethane although it is of course, as previously explained, susceptible for use with a number of similar materials as well, such as naphthalene, borneol, anthracene, or any volatile solid having a low intersolubility with a contained liquid at or above the melting point of the solid, from which In upper container treating hexachlorethane, for example, the valve is opened, that is, the plug 63 is positioned as shown in Fig. 1, the cover 68 is removed, and the hexachlorethane charged through the opening formed by the" tubular extension 66.

The material passes on down through the aperture 47 into the lower container. The charging is continued until the lower container is filled, and hexachlorethane added until the is preferably three-fourths filled, after which the addition of hexachlorethane is discontinued and the cover replaced and made tight.

Oil or any other suitable heating medium is then introducecL'as previously explained, into the jackets surrounding the containers until the hexachlorethane is melted and the water separated in a distinct line.

Liquefaction of the hexachlorethane will occur at around 184 C. and a pressure of approximately 160 pounds per square inch generated. The temperature and. pressure may be observed by a suitablethermometer and pressure gauge. The temperature maybe controlled by regulation of the liquid circulating through the heating jackets. It has been found that both the pressure and temperature will vary somewhat within certain limits according to the amount of impurities present:

In this state, the water layer is then removed through the pipe 73, the same either being rotated slowly toward, or positioned at the interface between the layers, the flow being controlled by a valve outside the container (not shown). After themajor portion of the water has been removed, communication between the containers is stopped by manipulation of the hand wheel 65, seating the plug 63 in the aperture 47. I

The contents of the chamber 35 may then be allowedto cool to around 185 C. when they may be blown through the conduit 53 by the introduction of air or other pressure medium through line 77, air preferably being admitted at about 175 pounds per square inch gauge pressure.

A line 79 having a valve 81 interposed therein is connected with the conduit 53 adapted to convey the material from the lower container to a cooling chamber 82 where the hexachlorethane may be subsequently obtained substan: tially free from moisture. When it is desired to remove the material from the container, such removal may be controlled by the valve 78.

After the charge has been blown from the chamber, the valve '78 is then closed and more heat applied to the charge in the upper chamber, making certain that the hexachlorethane is at least one to two degrees Centigrade above its melting point. Communication isthen reestablished by removal of the plug 63 from the aperture 47,, further introduction of air through the line '77 being discontinued, permittingthe molten hexachlorethane remaining in the. upper chamber to pass into the lower chamber together with any small amount of watenit may contain, preliminary to repeating the entire process. r l 1 There is accomplished by this invention a process and apparatus for removing contained liquids from volatile solvents having a low intersolubility therewith in the liquid phase without any appreciable loss of the normally solid material, and more especially a process .and. apparatus for drying hexachlorethane without loss of any substantial quantity of the compound.

While I have shown and described the preferred embodiment of my invention, I wish it to be understood that I do not confine myself to the precise details of construction herein set forth, by way of illustration, as it is apparent that many changes and variations may be made therein, by those skilled in the art, without departing from the spirit of the invention, or ex ceeding the scope of the appended claims.

I claim:

1. A process of separating a contained liquid and a solid without loss of the solid by vaporization, the solid having a high vapor pressure at room temperature and having a low intersolubility therewith and a different specific gravity from that of the liquid comprising heating within a closed space until the solid is liquefied and the liquefied solid and liquid separate due to their different specific gravities, and then withdrawing one of the separated products.

2. A process of removing contained liquid from a volatile solid without loss of the solid by vaporization, the solid having a high vapor pressure at room temperature and, the solid having a" diiferent specific gravity from that of the liquid, comprising liquefying the solid by heat in a closed space, and then withdrawing the liquid.

3. A process of removing a contained liquid .from a solid without loss of the solid by vaporization, the solid having a high vapor pressure at room temperature and having a low intersolubility therewith in the liquid phase comprising heating the solid above its melting point in a closed space, and drawing off one of the separated products.

4. A process of drying volatile water-contain ing solids without loss of the solid by vaporization, the solid having a high vapor pressure at room temperature and having a low intersolubility with Water in the liquid phase comprising heating the solid above its melting point in a closed space, and drawing off the water.

5. A process of drying hexachlorethane comprisingheating the hexachlorethane in a closed space until it is liquefied, and withdrawing one of the separated products.

6. A process of drying hexachlorethane comprising heating the hexachlorethane in a closed space until it is liquefied, and withdrawing the water.

7. A process of removing contained liquids from solids without loss of the solid by vaporization, the solid having a high vapor-pressure at room temperature and having a low intersolubility therewith comprising heating the solid in a closed space, until it liquefies, thus causing a separation into layers of the liquid and the liquefied solid, and drawing off the normally solid while in its liquid phase.

8. A process of separating a contained liquid from hexachlorethane comprising heating the hexachlorethane in a closed space until it liquefies, thus causing a separation into layers of the hexachlorethane and the liquid to be separated from the hexachlorethane, and then drawing oif the liquefied hexachlorethane.

9. A process of separating a contained liquid bility therewithand a different specific gravity from the liquid comprising heating the solid above its melting point in a plurality of superimposed communicating spaces, stopping communication between said spaces, and withdrawing the separated products.

10. A process of separating a contained liquid and a solid without loss of the solid by vaporization, the solidhaving a high vapor pressure at room temperature and, the contained liquid having a different specific gravity from the solid,

comprising heating the solid above its melting point in a plurality of superimposed communicating spaces, stopping communication between said spaces, and removing the solid while in liquid phase.

11. A process of separating a contained liquid and a solid without loss of the solid by vaporization, the solid having a high vapor pressure at room temperature and, the contained liquid having a low intersolubility with and a different tion, the solid having a high vapor pressure at room temperature and, the contained liquid having a low intersolubility with and a dilferent specific gravity from that of the solid when the solid is in its liquid phase, comprising heating the solid in a closed space until the normally solid material is in its liquid phase, separating the liquid from the liquefied solid, and drawing off the liquefied solid.

13. A process of separating a contained liquid I and a solid without loss of the solid by vaporization, the solid having a high vapor pressure :at room temperature and, the contained liquid having a low intersolubility with and a different specific gravity from that of the solid when the solid is liquefied, which comprises heating the solid in a closed space until the solid material is liquefied drawing oif most of the liquid, separating the liquefied solid from the remaining liquid, and drawing off the liquefied solid.

14. A process of separating a contained liquid and a solid without loss of the solid by vaporization, the solid having a high vapor pressure at room temperature and, the contained liquid having a low intersolubility with and a different specific gravity from that of the solid when the solid' is liquefied, which comprises heating the solid in a closed space until the solid is liquefied,

drawing oif most of the liquid, separating the I within two superimposed communicating spaces,

stopping communication between said spaces, withdrawing the hexachlorethane'from the lower space, and removing the water layerupon the hexachlorethane in the upper space.

ROLLAND D. MYERS; 

